Method of saturating fatty acids or their glycerids with hydrogen.



B. G. KAYSER.

METHOD OF SATURATING FATTY AO IDS 0B THEIR GLYOEBIDB WITH HYDBOGE] Arrmpulol mum 11:11.15, 1910.

1,008,474. 1 Pa tented Nov. 11, 1911.

UNITED STATES PATENT OFFICE.-

EDWIN CUNO KAYBEB, OI CINCINNATI, O HIO, ASSIGNOB TO THE PBOCTOB AND GAMBLE COMPANY, OF CINCINNATI, OHIO, A CORPOBATIOI OF OHIO.

IETHOD OI SATU'BATING FATTY ACIDS OB THEIR GLYCEBII IS WITH HYDROGEN.

Specification of Letters Patent. Pat gnted Nov, 14;, 1911.

Application filed February 18,1910. Serial No. 5443 30.

To all whom it may concern:

Be it known that I, EDWIN Cone KAYSER, a sub'ect of the King of Great Britain, and a resident of the city of Cincinnati, in the county of Hamilton and State of Ohio, United States of America, have invented -cert-ain new and useful Improvements in Methods for Saturatin Their Glycerids with the following is a specification.

It is by now well known that unsaturated fatty acids, their; glycerids or other esters, in the fluid state, can be made, to absorb gaseous hydrogen, until they become converted into the corresponding semi-saturated or saturated compounds, by the intervention of certain finely divided metals, nickel 'in particular. For that purpose, the nickelpowder is kept in suspension in the hot oil or fatty acid, while hydrogen gas is passed through, or otherwise brought in suitable contact with, the mixture.

In order to sufliciently expedite the transfer of hydrogen for practical purposes, considerable quantities of nickel have to be present. This metal must take the form of an almost impalpable powder and in conse- Fatty Acids or ydrogen, of which uence, when it comes to its se aration from t e product of reaction, it wil be found to form an almost im enetrable sediment on the filter cloth, a act greatly interfering with the technical applicability of the proc-' ess. Moreover, for reasons but imperfectly understood, but apparently dueto the deposition thereon of carbonaceous by-products, such pure metal soon loses its catalytic activity and cannot be made to repeatedly answer its pur ose.

In t e catalytic production of sulfuric acid, and in similar industrial processes, where reaction between gases is to be induced, it is customary to spread the catalytic metal or other catalyzer over fibrous ma: terials like asbestos, over fragments of brick or the like inert materials. Since the catalyst in these cases remains stationary, such measures are obviouslv necessary in order to facilitate the transverse movement. ofthe s through the catalyzer, or inorder to p uoe more contact 'thana mere passubstance such as kies'elguhr.

sage over a 'pulvero 1s layer of metal would afford, In the pm sent instance," however, when the metallic p irticles are already kept apart and readily accessible by their suspension in a liquid 1 medium, it would be considered unnecessarr to disseminate such metal over an inert vehicle and the presence of the latter would be judged more likely to impede than to iacilitate the reaction. I have, notwithstam ling this, ascertained, however, that nick1l firmly and evenly deposited upon a VOll minous, pulverous inert material exercises in a fluid medium a far more energetic acti In, and much longer retains its vitality tl ran an equal wei ht of pure metal procurable. The 111 zthod of thus depositin on or coating the )ulverous inert materia with the nickel powder forms no part of ,my present inventi )n, which relates to the use of such pulvero is nickelized material in the saturation of o ls and fats with hydrogen. It will, there: ore, be sufficient to state that in order to pn p'are my catal tic agent, I bring suitable s1 luble or inso uble comounds of nickel ii an appro riate manner into intimate-comb: nation wit an inert absorptive and comp aratively bulky mineral I then dry and comminute thl product, and reducing the powder thus 1: roduced with h drogen,

, a highly eflicient a! d reliable nicke ized, in-

ert pulverohs material is the result.

In order to carry out my process, I introduce into a suite ble closed receptacle a quantity of the mix zure of my fatty material and the ulverize l, nickelized inert support, and y mean: of paddles or stirrers, I thoroughly agitate the mixture while introducing the hydroge a. The vessel may either be filled with the har e, in which case the gas has to be atom ize within the fluid, or the vessel may be c nly partly filled, so as to permit the a 'tator or paddles to propel or project the c arge i ate a surrounding atmosnhere of hydrogen. By preference, the hydrogen is. supplied lnder ressure, but a certain amount is al'v eye a lowed to cont-inuously escape in 0rd er to carry ofi generated in the finest state of division Under suitable precautions, water gas or other gasmixture sufiiciently rich in hydrogen gas may be used in place of pure hydrogen. When pure h drogen is used, under artificial pressure, t e as outlet should be closed by a weighted valve, and the gas supply so regulated as to constantly maintam the desired pressure.

The temperature of the oil mixture may vary within considerable limits. A temperature from one hundred and fifty degrees centigrade to one hundred and sixty degrees centigrade will, as a rule, be found desirable.

The great technical advantage secured by my process in which the nickel powder is firmly and evenly distributed upon the voluminous, pulverous inert material, when mixed with the oil or fat to be treated, may in part be attributed to the ultra-division of the metal, attainable by suitable chemical incorporation, with the inert vehicle, wherein it approaches the colloidal state. It may, however, with equal force be ascribed to a direct, cooperation between metal and inert body, the latter, present in preponderating quantity and volume, absorbing the h drogen in the first instance and then yiel ing it to the metal, which in turn transmits it to the fatty body. The prolonged vitality of the catalyzer may on the other hand be due either to a modified action of the disseminated metal and to a diminished formation of by-products, or to the retention thereof by the inert vehicle, or finally to the more constant physical structure of the metallic particles. Whatever be the cause of the increased activity and prolonged vitality of the metalliferous pulverous catalyzer over the pure metal, the direct technical advantage attained by the change is sufiiciently conspicuous. This advantage is further advanced b two other factors,

v greatly pronounced w en using a vehicle. l1ke kieselguhr, namely the comparatively low specific gravity and the easy permea bility of the catalyzer. The former greatly .facilitates suspension in the surrounding and deodorizing action upon the material treated, far beyond that observed'w'ith an equal proportion of pure metal.

Suitable apparatus for carryin out the process is shown in the accompanying drawmg, in which Figure 1 isa vertical axial section; and F1g. 2 1s a vertical transverse section on the,

line IIII of Figi 1.

The apparatus i ustrated comprises a stathence returned by a l zer, a steam jacket 3, hydrogen supplyand ischarge-pipes 4, 5, and revolving wiregauze beaters or agitators 6, carried by a central shaft 7 journaled in stuffing-boxes 8 in the ends of the cylinder. Hydrogen is supplied to the compression-pump 9 through a pipe 10 having a three-way or other cook 11. The unabsorbed excess of hydrogen escaping from the drum through the pipe 5 passes a weighted relief-valve l2 and is tpipe. 13 to the pump.

The liquid mixture 0 oil and catalyzer to be treated in the cylinder is indicated by the line 14. The product is delivered through the tap 15 havlng the cook 16.

In practice, the oil to be hydrogenized, for example cotton-seed oil, is preferably charged into the cylinder through the manhole 2 to about-the level indicated. A relatively small amount of-the nickelized catalyzer, usually less than one per cent. by weight of the oil, is also introduced. The mixture is then heated by steam in the acket- 3 to a temperature of about 150 to 160 C. Hydrogen is pumped into the cylinder through the pipe 4, the unabsorbed excess escapin through the pipe 5 and relief-valve 12, an the wire-gauze beaters are set in motion. The heat, supply of hydrogen and agitation are continued. until the oil has been hydrogenized tothe desired degree, as shown by its consistency or by determination of its titre and iodin value, usually for several hours and until'it has been converted into a product which is solid or semi-solid when cold. The cock 16 is then opened, the mixture of hydrogenized oil and catalyzer is run out through the tap 15, and the catalyzer is filtered out for reuse.

What I claim as new, and of my inventionand desire to secure by Letters Patent, is

1. The rocess of h drogenizing fatty acids and t eir esters, w ich consists in agitating in the presence of hydrogen a heated mixture of the fatty acid or ester and a pul- Verulent catalyzer consisting of a light, vo-' luminous, finely-divided, inert support impregnated with an active metal, whereby the catalyzer is maintained in suspension and the acid or ester and hydrogen are brought heated mixture of the atty acid or ester and a pulverulent catalyzer-consisting of alight, vo

uminous, finely-divided, inert support impregnated with metallic nickel, whereby the catalyzer is maintained in suspension and the acid or ester and h drogen are brought into intimate contact wlth the active t-ionary horizontal cylinder 1, having a mansurfaces of said catalyzen 3. The process of hydrogenizing fatty inert support impregnated with an active acidsdaind their esters, which (iglnsists in remetal. peate ro'ectin or re e 'n into an m atmosp er (if 0051 ress ed hydr gen por- V EDWIN JUNO KAYSER' 5 tions of a heated mixture of the fatty acid Attest:

or ester and a pulverulent catalyzer con- ARTHUR H. Ev v ALD, sisting of alight, voluminous, finely-divided, EARL W. GRIFE N.

Correction id Letters Patent No. 1,008,474.

[t is hereby certified that the name of the assignee in Letters Patent- No. 1,008,474, granted November 14, 1911, upon the application of Edwin Uuno Kayser, of Cincinnati, Ohio, for an improvement in Methods of saturating Fatty Acids or Their Glvcerids With Hydrogen, was erroneously written and print ad The Proctor and Gamble Company, whereas it should have been written and pr Lnted The Procter and Gamble Company; and that the said Letters Patent should b1 read with this correction therein that the some may conform to the record of tie case in the Patent Ofi ice.

Signed and sealed this 16th day of January, A; Df, 191 2.

' C. C BILLINGS,

[sine] Acting Comm 88110110? of Patents. 

